CN115721775B - Composite modified biological hydrogel dressing and preparation process thereof - Google Patents
Composite modified biological hydrogel dressing and preparation process thereof Download PDFInfo
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Abstract
The invention provides a composite modified biological hydrogel dressing and a preparation process thereof. The hydrogel dressing is prepared from the following raw materials in parts by weight: 1-5 parts of modified hydrogel and 1.2-6 parts of simethicone; the modified hydrogel is prepared from the following raw materials in parts by weight: 10-30 parts of modified acrylic acid, 1-2 parts of chitosan, 0.5-1 part of cross-linking agent, 0.25-1 part of photoinitiator, 66-89 parts of purified water and 1-2 parts of thickener; the modified acrylic ester is prepared from the following raw materials in parts by weight: 2-5 parts of acrylic acid, 1-3 parts of a Acer aculeatum extract, 5-7 parts of a solid catalyst and 1-2 parts of a polymerization inhibitor. Compared with the market biogel, the composite modified biogel provided by the invention has the advantages of excellent antibacterial and bacteriostatic functions, good physical adsorption performance and self-crosslinking material characteristics at normal temperature and pressure, capability of rapidly forming gel on the surface of a wound so as to achieve the application value of rapid hemostasis, good biocompatibility, high specific tissue adhesion strength and the like.
Description
Technical Field
The invention belongs to the field of hydrogels, and particularly relates to a composite modified biological hydrogel dressing and a preparation process thereof.
Background
The commercial biohydrogels mainly comprise four classes: antibacterial hydrogel dressing, absorbent hydrogel dressing, smart hydrogel dressing and composite hydrogel dressing. The antibacterial hydrogel dressing is mainly used for preventing wound suppuration caused by bacterial infection possibly generated clinically, and has the advantages of prolonged healing time, serious and even sepsis-causing problems, and the like, so the wound dressing has the antibacterial and bacteriostatic functions. Absorbent hydrogel dressings have both physical and chemical adsorption. The medicine has the effects of adsorbing and stopping bleeding, has excellent performance in the aspect of medicine loading, and can release medicine factors when being applied to a human body through physical adsorption or chemical bond combination of certain medicine components, thereby playing a role in treatment. The intelligent hydrogel dressing is hydrogel which can generate sensitive response to external stimulus and integrates self-detection, self-judgment and self-response. The intelligent hydrogels studied at present mainly comprise memory self-repairing property, pH value responsiveness, double light responsiveness, heat/pH double responsiveness, strain sensitive hydrogels and the like. The method is mainly applied to tissue engineering scaffolds at present. The performance of a single material cannot meet the requirement of diversification in the wound healing process, so the composite hydrogel dressing with multiple functions has been correspondingly developed. The composite hydrogel dressing is more excellent than a single hydrogel dressing in the aspects of mechanical property, water permeability, air permeability, liquid absorption rate, moisture retention, bioactivity, biocompatibility and the like, can meet the requirements of different wound conditions, and has unique advantages in the field of medical dressings. The current market mainly uses the following raw material composite hydrogels, including: polyvinyl alcohol, polyacrylic acid, methacryloylated gelatin, and the like.
Hydrogel developed by the university of fowler's university was found by examining literature and patent related products, patent application number 201910238165.5: the self-healing hydrogel contains unmodified acrylic acid, the carboxyl contained in the self-healing hydrogel can cause secondary injury to wounds due to the oxidizing property of the self-healing hydrogel, and the prepared gel dressing has no specific adhesion performance to biological tissues, and can not be adhered to the surfaces of the tissues to stop bleeding rapidly when the gel dressing faces large wounds due to intermolecular hydrogen bonds. Hong et al prepared Matrix Gel hydrogel with excellent mechanical properties and wet tissue adhesiveness and rapid hemostasis by using methyl methacrylate modified hyaluronic acid as a raw material, wherein the modification reduces the damage of the material to biological tissues, but the material tissue is too single, has only single hemostatic property, and also has no specific adhesion property to tissues.
Disclosure of Invention
Aiming at the defects that the main stream polymer biogel in the market at present has single function, can not generate stable adhesion with biological tissues, has certain damage to the biological tissues and the like, the invention provides the composite modified biogel dressing which has excellent antibacterial and bacteriostatic functions, has good physical adsorption performance and self-crosslinking material characteristics at normal temperature and normal pressure compared with the market biogel, can rapidly form gel on the surface of a wound to achieve the application value of rapid hemostasis, and has the characteristics of good biocompatibility, high specific tissue adhesion strength and the like.
The invention also uses the Acer aculeatum to modify the acrylic acid, and the name of the Acer aculeatum Yao medicine is: hand-sticking wind is often used for symptoms such as wound bleeding cold compress, rheumatalgia and the like by Yao civilian use, while the Acer aculeatum extract is obtained by classifying and purifying Acer aculeatum which is not planted by artificial introduction through column chromatography and HPLC, and the extract has proved to have anti-inflammatory and antibacterial activities, has small side effects as a traditional Chinese medicine, has good application prospect, but cannot be applied better due to difficult purification and separation.
The technical scheme of the invention is as follows:
the composite modified hydrogel dressing of the invention is prepared from the following raw materials in parts by weight: 1-5 parts of modified hydrogel and 1.2-6 parts of simethicone; the modified hydrogel is prepared from the following raw materials in parts by weight: 10-30 parts of modified acrylic acid, 1-2 parts of chitosan, 0.5-1 part of cross-linking agent, 0.25-1 part of photoinitiator, 66-89 parts of purified water and 1-2 parts of thickener; the modified acrylic ester is prepared from the following raw materials in parts by weight: 2-5 parts of acrylic acid, 1-3 parts of a Acer aculeatum extract, 5-7 parts of a solid catalyst and 1-2 parts of a polymerization inhibitor; the Acer aculeatum extract is prepared from the following raw materials in parts by weight: 1-5 parts of Acer aculeatum, and 4-20 parts of 94-96% v/v ethanol solution.
The preparation method of the modified biological hydrogel dressing comprises the following steps:
(1) Preparation of Acer aculeatum extract: a. 1-5 parts of dried and crushed branches and leaves of Acer aculeatum, 4-20 parts of 94-96% v/v ethanol solution, soaking for 48-72h, collecting leaching liquor, repeating for 2-5 times, and combining the leaching liquor; b. distilling under reduced pressure at 40-60deg.C for 8-10 hr to obtain extract; c. drying in vacuum oven at 40-50deg.C for 48-72 hr to obtain extract.
Preferably, the preparation method of the Acer aculeatum extract comprises the following steps: a. 1 part of dried and crushed Acer aculeatum branches and leaves in the shade, 4 parts of 95% v/v ethanol solution, soaking for 72 hours, collecting leaching liquor, repeating for 2 times, and combining the leaching liquor; b. distilling under reduced pressure at 55deg.C for 10 hr to obtain extract; c. drying in vacuum oven at 50deg.C for 72 hr to obtain extract.
(2) Preparation of modified acrylic acid: a. adding 2-5 parts of acrylic acid into a three-neck flask according to parts by weight, transferring 1-3 parts of Acer aculeatum extract into an oil bath pot, connecting a condensing tube and introducing N 2 Or inert gas is used for keeping the reaction system to be filled with protective gas, magnetic stirring is started, and the rotating speed is controlled at 120 revolutions/min; b. adding 5-7 parts of solid catalyst and 1-2 parts of polymerization inhibitor after the solution is uniformly stirred; c. after being uniformly mixed, the heating temperature is started and controlled at 110-135 ℃, and the reaction time is controlled at 300-500min; c. after the reaction is completed, the reaction is cooled to room temperature, and insoluble matters are filtered to obtain the modified acrylic acid.
Preferably, the preparation method of the modified acrylic acid comprises the following steps: a. adding 2 parts of acrylic acid into a three-neck flask according to parts by weight, transferring 1 part of the Acer aculeatum extract into an oil bath pot, connecting a condensing tube and introducing N 2 The reaction system is kept to be filled with protective gas, magnetic stirring is started, and the rotating speed is controlled at 120 revolutions per minute; b. adding 5 parts of solid catalyst and 1 part of polymerization inhibitor after the solution is uniformly stirred; c. after being uniformly mixed, the heating temperature is started and controlled at 135 ℃, and the reaction time is controlled at 500min; c. and after the reaction is completed, cooling the mixture to room temperature, and filtering insoluble matters to obtain the modified acrylic acid solution.
(3) Preparation of modified biological hydrogel: a. taking 10-30 parts of modified acrylic acid, 1-2 parts of chitosan and 66-89 parts of purified water according to parts by weight, heating and stirring to dissolve and uniformly mix, wherein the heating temperature is controlled at 40-60 ℃, the stirring speed is 120-180 r/min, and the stirring time is 10-20min; b. then adding 1-2 parts of thickener, 0.5-1 part of cross-linking agent and 0.25-1 part of photoinitiator, and continuously stirring for 10-20min; c. after the mother solution is stirred uniformly, transferring the mother solution into surface dishes, adding 6-12ml of the solution into each surface dish, prepolymerizing for 30-60min at 30-40 ℃, and then curing by using an ultraviolet curing box, wherein the curing parameters are as follows: the curing time is 60-120min at 10-15W and 345-365nm, and the improved biological hydrogel can be obtained after curing is completed.
Preferably, the preparation method of the modified biological hydrogel comprises the following steps: a. according to the weight parts, 30 parts of modified acrylic acid, 2 parts of chitosan and 66 parts of purified water are taken, heated and stirred to be dissolved and uniformly mixed, the heating temperature is controlled at 60 ℃, the stirring speed is 120 r/min, and the stirring time is 20min; b. then adding 2 parts of thickener, 1 part of cross-linking agent and 1 part of photoinitiator, and continuously stirring for 20min; c. after the mother solution is stirred uniformly, transferring the mother solution to surface dishes, adding 12ml of the solution into each surface dish, prepolymerizing for 30min at 40 ℃, and then curing by using an ultraviolet curing box, wherein the curing parameters are as follows: the curing time is 90min at 12W and 365nm, and the improved biological hydrogel can be obtained after the curing is completed.
(4) Preparation of modified biological hydrogel dressing: a. cutting the cured modified biological hydrogel, and drying in a vacuum drying oven at 50-65deg.C for 120-180min; b. the dried biological hydrogel fragments are put into a ball mill for grinding, and the working parameters of the mill are as follows: 30-50Hz,720-1080 seconds; c. the ground gel powder is sieved by a 100-150 mesh sieve to obtain modified biological hydrogel powder; d. and uniformly mixing the ground hydrogel powder with simethicone to obtain the modified biological hydrogel dressing.
Preferably, the preparation method of the modified biological hydrogel dressing comprises the following steps: a. cutting the cured modified biological hydrogel, and drying in a vacuum drying oven at 65 ℃ for 180min; b. the dried biological hydrogel fragments are put into a ball mill for grinding, and the working parameters of the mill are as follows: 30Hz,720 seconds; c. passing the ground gel powder through a 150-mesh sieve to obtain biological hydrogel powder; d. and uniformly mixing the ground hydrogel powder with simethicone to obtain the modified biological hydrogel dressing.
The cross-linking agent is: acrylic acid-N-hydroxysuccinimide ester (AA-NHS), adipic acid-N-hydroxysuccinimide ester, bromoacetic acid-N-succinimidyl ester;
the solid catalyst is as follows: solid supported heteropolyacid catalyst PW 12 At least one of cation exchange resin and solid acid molecular sieve HSZM-5;
the photoinitiator is as follows: at least one of camphorquinone, alpha-ketoglutaric acid, irgacure 784 (basf visible light initiator 784);
the thickener is as follows: at least one of acacia, carrageenan, pectin and agar;
the polymerization inhibitor is as follows: hydroquinone, hydroquinone methyl ether, copper dibutyl dithiocarbamate, phenothiazine, manganese acetate;
The preparation process of the modified biological hydrogel dressing comprises the following steps: 1. pulverizing branches and leaves of Acer aculeatum, soaking in 95% v/v ethanol solution, distilling under reduced pressure, and vacuum drying to obtain Acer aculeatum extract; 2. transferring the obtained Acer aculeatum extract, acrylic acid, solid catalyst and polymerization inhibitor into a three-neck flask, modifying in an oil bath, and filtering insoluble substances after the reaction is completed to obtain modified acrylic acid solution; 3. adding the modified hydrogel solution into a beaker, adding chitosan, stirring the purified water for 20min, and controlling the rotation speed of a stirrer to be 120 r/min and the temperature to be 50 ℃;4. adding the cross-linking agent, the photoinitiator and the thickener into the chamber after stirring is completed, and continuously maintaining stirring for 20min;5. after being stirred uniformly, the mixture is transferred to a surface dish for prepolymerization for 30min at 40 ℃, and then is transferred to an ultraviolet curing box for ultraviolet curing, wherein the curing parameters are 12W and 365nm;6. after solidification, the hydrogel is sheared, dried, ground and sieved, and is mixed with the simethicone, thus obtaining the target biological hydrogel dressing.
The invention has the beneficial effects that:
(1) Compared with the market biogel, the composite modified biogel dressing provided by the invention has the advantages of excellent antibacterial and bacteriostatic functions, good physical adsorption performance, self-crosslinking material characteristics at normal temperature and normal pressure, capability of rapidly forming gel on the surface of a wound so as to achieve the application value of rapid hemostasis, good biocompatibility, high specific tissue adhesion strength and the like.
(2) The polyacrylic acid hydrogel dressing has self-crosslinking performance, can be self-crosslinked to form a gel layer at normal temperature and pressure, can form the gel layer on the wound surface in a self-crosslinking mode to achieve the hemostatic effect when the dressing is coated on the wound surface, and the crosslinking agent containing NHS groups can introduce NHS into a polyacrylic acid long chain, and the NHS groups can be covalently bonded with imine bonds on the biological tissue surface to stably fix the dressing on the tissue surface.
The chitosan and the Acer aculeatum extract which are doped with the chitosan can enable the polyacrylic acid hydrogel dressing to have better antibacterial, bacteriostatic and hemostatic capabilities, and meanwhile, the carboxyl of the modified polyacrylic acid hydrogel dressing has esterification reaction with the hydroxyl in the Acer aculeatum extract, so that the damage of the oxidization of the carboxyl to tissues and blood is greatly reduced. On the other hand, the chain extension effect generated by modification of the polyacrylic acid hydrogel dressing also increases the polymerization strength of the modified polyacrylic acid hydrogel, so that the modified polyacrylic acid hydrogel has more excellent mechanical properties to cope with different use environments.
Drawings
FIG. 1, infrared spectra before and after hydrogel modification;
FIG. 2 shows Raman spectra before and after modification of the hydrogel;
FIG. 3. T-peel tensile test plot;
FIG. 4 is a shear tensile test chart;
FIG. 5 is a plan tensile strength test chart;
FIG. 6 SEM image of the modified hydrogel powder;
FIG. 7. Polyacrylic acid powder;
FIG. 8. Modified polyacrylic acid powder;
Detailed Description
In order to make the technical scheme of the present invention better understood by those skilled in the art, the present invention will be further described in detail by means of specific examples
Example 1
The modified acrylic ester is prepared from the following raw materials in parts by weight: 2 parts of acrylic acid, 1 part of a Acer aculeatum extract, 5 parts of a solid catalyst and 1 part of a polymerization inhibitor;
the modified hydrogel is prepared from the following raw materials in parts by weight: 30 parts of modified acrylic acid, 2 parts of chitosan, 1 part of cross-linking agent, 0.5 part of photoinitiator, 66 parts of purified water and 2 parts of thickening agent;
the modified hydrogel dressing is prepared from the following raw materials in parts by weight: 1 part of modified hydrogel and 1.2 parts of simethicone;
the preparation method of the biological hydrogel dressing comprises the following steps:
1. preparation of Acer aculeatum extract: a. 1 part of dried and crushed Acer aculeatum branches and leaves in the shade, 4 parts of 95% v/v ethanol solution, soaking for 72 hours, collecting leaching liquor, repeating for 2 times, and combining the leaching liquor; b. distilling under reduced pressure at 55deg.C for 10 hr to obtain extract; c. drying in vacuum oven at 50deg.C for 72 hr to obtain extract.
2. Preparation of modified acrylic acid: a. adding 2 parts of acrylic acid into a three-neck flask according to parts by weight, transferring 1 part of the Acer aculeatum extract into an oil bath pot, connecting a condensing tube and introducing N 2 The reaction system is kept to be filled with protective gas, magnetic stirring is started, and the rotating speed is controlled at 120 revolutions per minute; b. adding 5 parts of solid catalyst and 1 part of polymerization inhibitor after the solution is uniformly stirred; c. after being uniformly mixed, the heating temperature is started and controlled at 135 ℃, and the reaction time is controlled at 500min; c. after the reaction is completed, the reaction is cooled to room temperature, and insoluble matters are filtered to obtain the modified acrylic acid.
3. Preparation of modified biological hydrogel: a. according to the weight parts, 30 parts of modified acrylic acid, 2 parts of chitosan and 66 parts of purified water are taken, heated and stirred to be dissolved and uniformly mixed, the heating temperature is controlled at 60 ℃, the stirring speed is 120 r/min, and the stirring time is 20min; b. then adding 2 parts of thickener and 1 part of cross-linking agent, and continuously stirring for 20min by 0.5 part of photoinitiator; c. after the mother solution is stirred uniformly, transferring the mother solution to surface dishes, adding 12ml of the solution into each surface dish, prepolymerizing for 30min at 40 ℃, and then curing by using an ultraviolet curing box, wherein the curing parameters are as follows: the curing time is 90min at 12W and 365nm, and the improved biological hydrogel can be obtained after the curing is completed.
4. Preparation of modified biological hydrogel dressing: a. cutting 1 part of modified biological hydrogel after curing is completed, and then drying in a vacuum drying oven at 65 ℃ for 180min; b. the dried biological hydrogel fragments are put into a ball mill for grinding, and the working parameters of the mill are as follows: 30Hz,720 seconds; c. the ground gel powder passes through a 150-mesh sieve to obtain modified biological hydrogel powder; d. and uniformly mixing the ground hydrogel powder with 1.2 parts of dimethyl silicone oil to obtain the modified biological hydrogel dressing.
The solid catalyst used was: PW (pseudo wire) 12 ；
The polymerization inhibitor used is: phenothiazine;
the cross-linking agent is: acrylic acid-N-hydroxysuccinimide ester;
the photoinitiator is as follows: alpha-ketoglutaric acid;
the thickener is as follows: gelatin;
the preparation process of the modified biological hydrogel dressing comprises the following steps: 1. pulverizing branches and leaves of Acer aculeatum, soaking in 95% v/v ethanol solution, distilling under reduced pressure, and vacuum drying to obtain Acer aculeatum extract; 2. mixing the obtained Acer aculeatum extract with acrylic acid and PW 12 Transferring the phenothiazine and the phenothiazine into a three-neck flask, modifying in an oil bath pot, and filtering insoluble substances after the reaction is finished to obtain a modified acrylic acid solution; 3. adding the modified hydrogel solution into a beaker, adding chitosan and purified water, and stirring for 20min;4. adding acrylic acid-N-hydroxysuccinimide ester, alpha-ketoglutaric acid and gelatin into the chamber after stirring is completed, and continuously maintaining stirring for 20min;5. uniformly stirring, transferring to a surface dish, prepolymerizing for 30min at 40 ℃, and transferring to an ultraviolet curing box for ultraviolet curing; 6. after solidification, the hydrogel is sheared, dried, ground and sieved, and is mixed with the simethicone, thus obtaining the target biological hydrogel dressing.
Example 2
The Acer aculeatum extract is prepared from the following raw materials in parts by weight: 1 part of Acer aculeatum, 4 parts of 95% v/v ethanol solution;
the modified acrylic ester is prepared from the following raw materials in parts by weight: 2 parts of acrylic acid, 1 part of a calyx seu fructus physalis extract, 5 parts of a solid catalyst and 2 parts of a polymerization inhibitor;
the modified hydrogel is prepared from the following raw materials in parts by weight: 10 parts of modified acrylic acid, 2 parts of chitosan, 1 part of cross-linking agent, 0.5 part of photoinitiator, 89 parts of purified water and 2 parts of thickening agent;
the modified hydrogel dressing is prepared from the following raw materials in parts by weight: 1 part of modified hydrogel and 1.2 parts of simethicone;
the preparation method of the biological hydrogel dressing comprises the following steps:
1. preparation of Acer aculeatum extract: a. 1 part of dried and crushed Acer aculeatum branches and leaves in the shade, 4 parts of 95% v/v ethanol solution, soaking for 72 hours, collecting leaching liquor, repeating for 2 times, and combining the leaching liquor; b. distilling under reduced pressure at 55deg.C for 10 hr to obtain extract; c. drying in vacuum oven at 50deg.C for 72 hr to obtain extract.
2. Preparation of modified acrylic acid: a. adding 2 parts of acrylic acid into a three-neck flask according to parts by weight, transferring 1 part of the Acer aculeatum extract into an oil bath pot, connecting a condensing tube and introducing N 2 The reaction system is kept to be filled with protective gas, magnetic stirring is started, and the rotating speed is controlled at 120 revolutions per minute; b. adding 5 parts of solid catalyst and 1 part of polymerization inhibitor after the solution is uniformly stirred; c. after being uniformly mixed, the heating temperature is started and controlled at 135 ℃, and the reaction time is controlled at 500min; c. after the reaction is completed, the reaction is cooled to room temperature, and insoluble matters are filtered to obtain the modified acrylic acid.
3. Preparation of modified biological hydrogel: a. taking 10 parts by weight of modified acrylic acid, 2 parts by weight of chitosan and 86 parts by weight of purified water, heating and stirring to dissolve and uniformly mix, controlling the heating temperature to 60 ℃, the stirring speed to 120 r/min and the stirring time to 20min; b. then adding 2 parts of thickener and 1 part of cross-linking agent, and continuously stirring for 20min by 0.5 part of photoinitiator; c. after the mother solution is stirred uniformly, transferring the mother solution to surface dishes, adding 12ml of the solution into each surface dish, prepolymerizing for 30min at 40 ℃, and then curing by using an ultraviolet curing box, wherein the curing parameters are as follows: the curing time is 90min at 12W and 365nm, and the improved biological hydrogel can be obtained after the curing is completed.
4. Preparation of modified biological hydrogel dressing: a. cutting a part of cured modified biological hydrogel, and then placing the cut modified biological hydrogel in a vacuum drying oven for drying at 65 ℃ for 180min; b. the dried biological hydrogel fragments are put into a ball mill for grinding, and the working parameters of the mill are as follows: 30Hz,720 seconds; c. the ground gel powder passes through a 150-mesh sieve to obtain modified biological hydrogel powder; d. and uniformly mixing the ground hydrogel powder with 1.2 parts of simethicone to obtain the modified biological hydrogel dressing.
The solid catalyst used was: PW (pseudo wire) 12 ；
The polymerization inhibitor used is: phenothiazine;
the cross-linking agent is: adipic acid-N-hydroxysuccinimide;
the photoinitiator is as follows: alpha-ketoglutaric acid;
the thickener is as follows: gelatin;
the preparation process of the modified biological hydrogel dressing comprises the following steps: 1. pulverizing branches and leaves of Acer aculeatum, soaking in 95% v/v ethanol solution, distilling under reduced pressure, and vacuum drying to obtain Acer aculeatum extract; 2. mixing the obtained Acer aculeatum extract with acrylic acid and PW 12 Transferring the phenothiazine and the phenothiazine into a three-neck flask, modifying in an oil bath pot, and filtering insoluble substances after the reaction is finished to obtain a modified acrylic acid solution; 3. adding the modified hydrogel solution into a beaker, adding chitosan, and stirring the purified water for 20min;4. adding adipic acid-N-hydroxysuccinimide ester, alpha-ketoglutaric acid and gelatin into the chamber after stirring is completed, and continuously maintaining stirring for 20min;5. uniformly stirring, transferring to a surface dish, prepolymerizing for 30min at 40 ℃, and transferring to an ultraviolet curing box for ultraviolet curing; 6. after solidification, the hydrogel is sheared, dried, ground and sieved, and is mixed with the simethicone, thus obtaining the target biological hydrogel dressing.
Example 3
The Acer aculeatum extract is prepared from the following raw materials in parts by weight: 1 part of Acer aculeatum, 4 parts of 95% v/v ethanol solution;
the modified acrylic ester is prepared from the following raw materials in parts by weight: 2 parts of acrylic acid, 1 part of a Acer aculeatum extract, 5 parts of a solid catalyst and 1 part of a polymerization inhibitor;
the modified hydrogel is prepared from the following raw materials in parts by weight: 30 parts of modified acrylic acid, 2 parts of chitosan, 1 part of cross-linking agent, 0.5 part of photoinitiator, 66 parts of purified water and 2 parts of thickening agent;
the modified hydrogel dressing is prepared from the following raw materials in parts by weight: 1 part of modified hydrogel and 1.2 parts of simethicone;
the preparation method of the biological hydrogel dressing comprises the following steps:
1. preparation of Acer aculeatum extract: a. 1 part of dried and crushed Acer aculeatum branches and leaves in the shade, 4 parts of 95% v/v ethanol solution, soaking for 72 hours, collecting leaching liquor, repeating for 2 times, and combining the leaching liquor; b. distilling under reduced pressure at 55deg.C for 10 hr to obtain extract; c. drying in vacuum oven at 50deg.C for 72 hr to obtain extract.
2. Preparation of modified acrylic acid: a. adding 2 parts of acrylic acid into a three-neck flask according to parts by weight, transferring 1 part of the Acer aculeatum extract into an oil bath pot, connecting a condensing tube and introducing N 2 The reaction system is kept to be filled with protective gas, magnetic stirring is started, and the rotating speed is controlled at 120 revolutions per minute; b. adding 5 parts of solid catalyst and 1 part of polymerization inhibitor after the solution is uniformly stirred; c. after being uniformly mixed, the heating temperature is started and controlled at 135 ℃, and the reaction time is controlled at 500min; c. after the reaction is completed, the reaction is cooled to room temperature, and insoluble matters are filtered to obtain the modified acrylic acid.
3. Preparation of modified biological hydrogel: a. taking 10 parts by weight of modified acrylic acid, 2 parts by weight of chitosan and 86 parts by weight of purified water, heating and stirring to dissolve and uniformly mix, controlling the heating temperature to 60 ℃, the stirring speed to 120 r/min and the stirring time to 20min; b. then adding 2 parts of thickener and 1 part of cross-linking agent, and continuously stirring for 20min by 0.5 part of photoinitiator; c. after the mother solution is stirred uniformly, transferring the mother solution to surface dishes, adding 12ml of the solution into each surface dish, prepolymerizing for 30min at 40 ℃, and then curing by using an ultraviolet curing box, wherein the curing parameters are as follows: the curing time is 90min at 12W and 365nm, and the improved biological hydrogel can be obtained after the curing is completed.
4. Preparation of modified biological hydrogel dressing: a. shearing 1 part of the cured modified biological hydrogel, and then drying in a vacuum drying oven at 65 ℃ for 180min; b. the dried biological hydrogel fragments are put into a ball mill for grinding, and the working parameters of the mill are as follows: 30Hz,720 seconds; c. the ground gel powder passes through a 150-mesh sieve to obtain modified biological hydrogel powder; d. and uniformly mixing the ground hydrogel powder with 1.2 parts of simethicone to obtain the modified biological hydrogel dressing.
The solid catalyst used was: PW (pseudo wire) 12 ；
The polymerization inhibitor used is: phenothiazine;
the cross-linking agent is: acrylic acid-N-hydroxysuccinimide ester;
the photoinitiator is as follows: alpha-ketoglutaric acid;
the thickener is as follows: gelatin;
the preparation process of the modified biological hydrogel dressing comprises the following steps: 1. pulverizing branches and leaves of Acer aculeatum, soaking in 95% v/v ethanol solution, distilling under reduced pressure, and vacuum drying to obtain Acer aculeatum extract; 2. mixing the obtained Acer aculeatum extract with acrylic acid and PW 12 Transferring the phenothiazine and the phenothiazine into a three-neck flask, modifying in an oil bath pot, and filtering insoluble substances after the reaction is finished to obtain a modified acrylic acid solution; 3. adding the modified hydrogel solution into a beaker, adding chitosan and purified water, and stirring for 20min;4. adding acrylic acid-N-hydroxysuccinimide ester, alpha-ketoglutaric acid and gelatin into the chamber after stirring is completed, and continuously maintaining stirring for 20min;
5. uniformly stirring, transferring to a surface dish, prepolymerizing for 30min at 40 ℃, and transferring to an ultraviolet curing box for ultraviolet curing;
6. after solidification, the hydrogel is sheared, dried, ground and sieved, and is mixed with the simethicone, thus obtaining the target biological hydrogel dressing.
Example 4
The Acer aculeatum extract is prepared from the following raw materials in parts by weight: 1 part of Acer aculeatum, 4 parts of 95% v/v ethanol solution;
the modified acrylic ester is prepared from the following raw materials in parts by weight: 2 parts of acrylic acid, 1 part of a Acer aculeatum extract, 5 parts of a solid catalyst and 1 part of a polymerization inhibitor;
the modified hydrogel is prepared from the following raw materials in parts by weight: 30 parts of modified acrylic acid, 2 parts of chitosan, 1 part of cross-linking agent, 0.5 part of photoinitiator, 66 parts of purified water and 2 parts of thickening agent;
the modified hydrogel dressing is prepared from the following raw materials in parts by weight: 1 part of modified hydrogel and 1.2 parts of simethicone;
the preparation method of the biological hydrogel dressing comprises the following steps:
1. preparation of Acer aculeatum extract: a. 1 part of dried and crushed Acer aculeatum branches and leaves in the shade, 4 parts of 95% v/v ethanol solution, soaking for 72 hours, collecting leaching liquor, repeating for 2 times, and combining the leaching liquor; b. distilling under reduced pressure at 55deg.C for 10 hr to obtain extract; c. drying in vacuum oven at 50deg.C for 72 hr to obtain extract.
2. Preparation of modified acrylic acid: a. adding 2 parts of acrylic acid into a three-neck flask according to parts by weight, transferring 2 parts of Acer aculeatum extract into an oil bath pot, connecting a condensing tube and introducing N 2 The reaction system is kept to be filled with protective gas, magnetic stirring is started, and the rotating speed is controlled at 120 revolutions per minute; b. adding 5 parts of solid catalyst and 1 part of polymerization inhibitor after the solution is uniformly stirred; c. after being uniformly mixed, the heating temperature is started and controlled at 135 ℃, and the reaction time is controlled at 500min; c. after the reaction is completed, the reaction is cooled to room temperature, and insoluble matters are filtered to obtain the modified acrylic acid.
3. Preparation of modified biological hydrogel: a. according to the weight parts, 30 parts of modified acrylic acid, 2 parts of chitosan and 66 parts of purified water are taken, heated and stirred to be dissolved and uniformly mixed, the heating temperature is controlled at 60 ℃, the stirring speed is 120 r/min, and the stirring time is 20min; b. then adding 2 parts of thickener and 1 part of cross-linking agent, and continuously stirring for 20min by 0.5 part of photoinitiator; c. after the mother solution is stirred uniformly, transferring the mother solution to surface dishes, adding 12ml of the solution into each surface dish, prepolymerizing for 30min at 40 ℃, and then curing by using an ultraviolet curing box, wherein the curing parameters are as follows: the curing time is 90min at 12W and 365nm, and the improved biological hydrogel can be obtained after the curing is completed.
4. Preparation of modified biological hydrogel dressing: a. cutting the cured modified biological hydrogel, and drying in a vacuum drying oven at 65 ℃ for 180min; b. the dried biological hydrogel fragments are put into a ball mill for grinding, and the working parameters of the mill are as follows: 30Hz,720 seconds; c. the ground gel powder passes through a 150-mesh sieve to obtain modified biological hydrogel powder; d. and uniformly mixing the ground hydrogel powder with 30 parts of simethicone to obtain the modified biological hydrogel dressing.
The solid catalyst used was: PW (pseudo wire) 12
The polymerization inhibitor used is: phenothiazines
The cross-linking agent is: bromoacetic acid-N-succinimidyl ester;
the photoinitiator is as follows: alpha-ketoglutaric acid;
the thickener is as follows: gelatin
The preparation process of the modified biological hydrogel dressing comprises the following steps: 1. pulverizing branches and leaves of Acer aculeatum, soaking in 95% v/v ethanol solution, distilling under reduced pressure, and vacuum drying to obtain Acer aculeatum extract; 2. mixing the obtained Acer aculeatum extract with acrylic acid and PW 12 Transferring the phenothiazine and the phenothiazine into a three-neck flask, modifying in an oil bath pot, and filtering insoluble substances after the reaction is finished to obtain a modified acrylic acid solution; 3. adding the modified hydrogel solution into a beaker, adding chitosan, stirring the purified water for 20min, and controlling the rotation speed of a stirrer to be 120 r/min and the temperature to be 50 ℃;4. adding bromoacetic acid-N-succinimidyl ester, alpha-ketoglutaric acid and gelatin into the chamber after stirring is completed, and continuously maintaining stirring for 20min;5. uniformly stirring, transferring to a surface dish, prepolymerizing for 30min at 40 ℃, and transferring to an ultraviolet curing box for ultraviolet curing; 6. after solidification, the hydrogel is sheared, dried, ground and sieved, and is mixed with the simethicone, thus obtaining the target biological hydrogel dressing.
Example 5
The Acer aculeatum extract is prepared from the following raw materials in parts by weight: 1 part of Acer aculeatum, 4 parts of 95% v/v ethanol solution;
the modified acrylic ester is prepared from the following raw materials in parts by weight: 2 parts of acrylic acid, 1 part of a Acer aculeatum extract, 5 parts of a solid catalyst and 1 part of a polymerization inhibitor;
the modified hydrogel is prepared from the following raw materials in parts by weight: 30 parts of modified acrylic acid, 2 parts of chitosan, 1 part of cross-linking agent, 0.5 part of photoinitiator, 66 parts of purified water and 2 parts of thickening agent;
the modified hydrogel dressing is prepared from the following raw materials in parts by weight: 1 part of modified hydrogel and 1.2 parts of simethicone;
the preparation method of the biological hydrogel dressing comprises the following steps:
1. preparation of Acer aculeatum extract: a. 1 part of dried and crushed Acer aculeatum branches and leaves in the shade, 4 parts of 95% v/v ethanol solution, soaking for 72 hours, collecting leaching liquor, repeating for 2 times, and combining the leaching liquor; b. distilling under reduced pressure at 55deg.C for 10 hr to obtain extract; c. drying in vacuum oven at 50deg.C for 72 hr to obtain extract.
2. Preparation of modified acrylic acid: a. adding 2 parts of acrylic acid into a three-neck flask according to parts by weight, transferring 1 part of the Acer aculeatum extract into an oil bath pot, connecting a condensing tube and introducing N 2 The reaction system is kept to be filled with protective gas, magnetic stirring is started, and the rotating speed is controlled at 120 revolutions per minute; b. adding 5 parts of solid catalyst and 1 part of polymerization inhibitor after the solution is uniformly stirred; c. after being uniformly mixed, the heating temperature is started and controlled at 135 ℃, and the reaction time is controlled at 500min; c. after the reaction is completed, the reaction is cooled to room temperature, and insoluble matters are filtered to obtain the modified acrylic acid.
3. Preparation of modified biological hydrogel: a. according to the weight parts, 30 parts of modified acrylic acid, 2 parts of chitosan and 66 parts of purified water are taken, heated and stirred to be dissolved and uniformly mixed, the heating temperature is controlled at 60 ℃, the stirring speed is 120 r/min, and the stirring time is 20min; b. then adding 2 parts of thickener and 1 part of cross-linking agent, and continuously stirring for 20min by 0.5 part of photoinitiator; c. after the mother solution is stirred uniformly, transferring the mother solution to surface dishes, adding 12ml of the solution into each surface dish, prepolymerizing for 30min at 40 ℃, and then curing by using an ultraviolet curing box, wherein the curing parameters are as follows: the curing time is 90min at 12W and 365nm, and the improved biological hydrogel can be obtained after the curing is completed.
4. Preparation of modified biological hydrogel dressing: a. cutting the cured modified biological hydrogel, and drying in a vacuum drying oven at 65 ℃ for 180min; b. the dried biological hydrogel fragments are put into a ball mill for grinding, and the working parameters of the mill are as follows: 30Hz,720 seconds; c. the ground gel powder passes through a 150-mesh sieve to obtain modified biological hydrogel powder; d. and uniformly mixing the ground hydrogel powder with 30 parts of simethicone to obtain the modified biological hydrogel dressing.
The solid catalyst used was: PW (pseudo wire) 12
The polymerization inhibitor used is: phenothiazines
The cross-linking agent is: n, N' -methylenebisacrylamide;
the photoinitiator is as follows: alpha-ketoglutaric acid;
the thickener is as follows: gelatin
The preparation process of the modified biological hydrogel dressing comprises the following steps: 1. pulverizing branches and leaves of Acer aculeatum, soaking in 95% v/v ethanol solution, distilling under reduced pressure, and vacuum drying to obtain Acer aculeatum extract; 2. mixing the obtained Acer aculeatum extract with acrylic acid and PW 12 Transferring the phenothiazine and the phenothiazine into a three-neck flask, modifying in an oil bath pot, and filtering insoluble substances after the reaction is finished to obtain a modified acrylic acid solution; 3. adding the modified hydrogel solution into a beaker, adding chitosan, and stirring the purified water for 20min;4. adding N, N' -methylene bisacrylamide, alpha-ketoglutaric acid and gelatin into the chamber after stirring is completed, and continuously maintaining stirring for 20min;5. uniformly stirring, transferring to a surface dish, prepolymerizing for 30min at 40 ℃, and transferring to an ultraviolet curing box for ultraviolet curing; 6. after solidification, the hydrogel is sheared, dried, ground and sieved, and is mixed with the simethicone, thus obtaining the target biological hydrogel dressing.
Example 6
The Acer aculeatum extract is prepared from the following raw materials in parts by weight: 1 part of Acer aculeatum, 4 parts of 95% v/v ethanol solution;
the modified acrylic ester is prepared from the following raw materials in parts by weight: 2 parts of acrylic acid, 1 part of a Acer aculeatum extract, 5 parts of a solid catalyst and 1 part of a polymerization inhibitor;
the modified hydrogel is prepared from the following raw materials in parts by weight: 5 parts of modified acrylic acid, 2 parts of chitosan, 1 part of cross-linking agent, 0.5 part of photoinitiator, 66 parts of purified water and 2 parts of thickening agent;
the modified hydrogel dressing is prepared from the following raw materials in parts by weight: 1 part of modified hydrogel and 1.2 parts of simethicone;
the preparation method of the biological hydrogel dressing comprises the following steps:
1. preparation of Acer aculeatum extract: a. 1 part of dried and crushed Acer aculeatum branches and leaves in the shade, 4 parts of 95% v/v ethanol solution, soaking for 72 hours, collecting leaching liquor, repeating for 2 times, and combining the leaching liquor; b. distilling under reduced pressure at 55deg.C for 10 hr to obtain extract; c. drying in vacuum oven at 50deg.C for 72 hr to obtain extract.
2. Preparation of modified acrylic acid: a. adding 2 parts of acrylic acid into a three-neck flask according to parts by weight, transferring 1 part of the Acer aculeatum extract into an oil bath pot, connecting a condensing tube and introducing N 2 The reaction system is kept to be filled with protective gas, magnetic stirring is started, and the rotating speed is controlled at 120 revolutions per minute; b. adding 5 parts of solid catalyst and 1 part of polymerization inhibitor after the solution is uniformly stirred; c. after being uniformly mixed, the heating temperature is started and controlled at 135 ℃, and the reaction time is controlled at 500min; c. after the reaction is completed, the reaction is cooled to room temperature, and insoluble matters are filtered to obtain the modified acrylic acid.
3. Preparation of modified biological hydrogel: a. taking 5 parts by weight of modified acrylic acid, 2 parts by weight of chitosan and 66 parts by weight of purified water, heating and stirring to dissolve and uniformly mix, controlling the heating temperature to 60 ℃, the stirring speed to 120 r/min and the stirring time to 20min; b. then adding 2 parts of thickener and 1 part of cross-linking agent, and continuously stirring for 20min by 0.5 part of photoinitiator; c. after the mother solution is stirred uniformly, transferring the mother solution to surface dishes, adding 12ml of the solution into each surface dish, prepolymerizing for 30min at 40 ℃, and then curing by using an ultraviolet curing box, wherein the curing parameters are as follows: the curing time is 90min at 12W and 365nm, and the improved biological hydrogel can be obtained after the curing is completed.
4. Preparation of modified biological hydrogel dressing: a. cutting the cured modified biological hydrogel, and drying in a vacuum drying oven at 65 ℃ for 180min; b. the dried biological hydrogel fragments are put into a ball mill for grinding, and the working parameters of the mill are as follows: 30Hz,720 seconds; c. the ground gel powder passes through a 150-mesh sieve to obtain modified biological hydrogel powder; d. and uniformly mixing the ground hydrogel powder with 30 parts of simethicone to obtain the modified biological hydrogel dressing.
The solid catalyst used was: PW (pseudo wire) 12
The polymerization inhibitor used is: phenothiazines
The cross-linking agent is: acrylic acid-N-hydroxysuccinimide ester;
the photoinitiator is as follows: alpha-ketoglutaric acid;
the thickener is as follows: gelatin
The preparation process of the modified biological hydrogel dressing comprises the following steps: 1. pulverizing branches and leaves of Acer aculeatum, soaking in 95% v/v ethanol solution, distilling under reduced pressure, and vacuum drying to obtain Acer aculeatum extract; 2. mixing the obtained Acer aculeatum extract with acrylic acid and PW 12 Transferring the phenothiazine and the phenothiazine into a three-neck flask, modifying in an oil bath pot, and filtering insoluble substances after the reaction is finished to obtain a modified acrylic acid solution; 3. adding the modified hydrogel solution into a beaker, adding chitosan, and stirring the purified water for 20min;4. adding acrylic acid-N-hydroxysuccinimide ester, alpha-ketoglutaric acid and gelatin into the chamber after stirring is completed, and continuously maintaining stirring for 20min;5. uniformly stirring, transferring to a surface dish, prepolymerizing for 30min at 40 ℃, and transferring to an ultraviolet curing box for ultraviolet curing; 6. after solidification, the hydrogel is sheared, dried, ground and sieved, and is mixed with the simethicone, thus obtaining the target biological hydrogel dressing.
Example 7
The Acer aculeatum extract is prepared from the following raw materials in parts by weight: 1 part of Acer aculeatum, 4 parts of 95% v/v ethanol solution;
the modified acrylic ester is prepared from the following raw materials in parts by weight: 2 parts of acrylic acid, 1 part of a Acer aculeatum extract, 5 parts of a solid catalyst and 1 part of a polymerization inhibitor;
the modified hydrogel is prepared from the following raw materials in parts by weight: 40 parts of modified acrylic acid, 1 part of chitosan, 0.5 part of cross-linking agent, 0.5 part of photoinitiator, 66 parts of purified water and 2 parts of thickening agent;
the modified hydrogel dressing is prepared from the following raw materials in parts by weight: 1 part of modified hydrogel and 1.2 parts of simethicone;
the preparation method of the biological hydrogel dressing comprises the following steps:
1. preparation of Acer aculeatum extract: a. 1 part of dried and crushed Acer aculeatum branches and leaves in the shade, 4 parts of 95% v/v ethanol solution, soaking for 72 hours, collecting leaching liquor, repeating for 2 times, and combining the leaching liquor; b. distilling under reduced pressure at 55deg.C for 10 hr to obtain extract; c. drying in vacuum oven at 50deg.C for 72 hr to obtain extract.
2. Preparation of modified acrylic acid: a. adding 2 parts of acrylic acid into a three-neck flask according to parts by weight, transferring 1 part of the Acer aculeatum extract into an oil bath pot, connecting a condensing tube and introducing N 2 The reaction system is kept to be filled with protective gas, magnetic stirring is started, and the rotating speed is controlled at 120 revolutions per minute; b. adding 5 parts of solid catalyst and 1 part of polymerization inhibitor after the solution is uniformly stirred; c. after being uniformly mixed, the heating temperature is started and controlled at 135 ℃, and the reaction time is controlled at 500min; c. after the reaction is completed, the reaction is cooled to room temperature, and insoluble matters are filtered to obtain the modified acrylic acid.
3. Preparation of modified biological hydrogel: a. according to the weight parts, 40 parts of modified acrylic acid, 2 parts of chitosan and 66 parts of purified water are taken, heated and stirred to be dissolved and uniformly mixed, the heating temperature is controlled at 60 ℃, the stirring speed is 120 r/min, and the stirring time is 20min; b. then adding 2 parts of thickener and 1 part of cross-linking agent, and continuously stirring for 20min by 0.5 part of photoinitiator; c. after the mother solution is stirred uniformly, transferring the mother solution to surface dishes, adding 12ml of the solution into each surface dish, prepolymerizing for 30min at 40 ℃, and then curing by using an ultraviolet curing box, wherein the curing parameters are as follows: the curing time is 90min at 12W and 365nm, and the improved biological hydrogel can be obtained after the curing is completed.
4. Preparation of modified biological hydrogel dressing: a. cutting the cured modified biological hydrogel, and drying in a vacuum drying oven at 65 ℃ for 180min; b. the dried biological hydrogel fragments are put into a ball mill for grinding, and the working parameters of the mill are as follows: 30Hz,720 seconds; c. the ground gel powder passes through a 150-mesh sieve to obtain modified biological hydrogel powder; d. and uniformly mixing the ground hydrogel powder with 30 parts of simethicone to obtain the modified biological hydrogel dressing.
The solid catalyst used was: PW (pseudo wire) 12
The polymerization inhibitor used is: phenothiazines
The cross-linking agent is: acrylic acid-N-hydroxysuccinimide ester;
the photoinitiator is as follows: alpha-ketoglutaric acid;
the thickener is as follows: gelatin
The preparation process of the modified biological hydrogel dressing comprises the following steps: 1. pulverizing branches and leaves of Acer aculeatum, soaking in 95% v/v ethanol solution, distilling under reduced pressure, and vacuum drying to obtain Acer aculeatum extract; 2. mixing the obtained Acer aculeatum extract with acrylic acid and PW 12 Transferring the phenothiazine and the phenothiazine into a three-neck flask, modifying in an oil bath pot, and filtering insoluble substances after the reaction is finished to obtain a modified acrylic acid solution; 3. adding the modified hydrogel solution into a beaker, adding chitosan, and stirring the purified water for 20min;4. adding acrylic acid-N-hydroxysuccinimide ester, alpha-ketoglutaric acid and gelatin into the chamber after stirring is completed, and continuously maintaining stirring for 20min;5. uniformly stirring, transferring to a surface dish, prepolymerizing for 30min at 40 ℃, and transferring to an ultraviolet curing box for ultraviolet curing; 6. after solidification, the hydrogel is sheared, dried, ground and sieved, and is mixed with the simethicone, thus obtaining the target biological hydrogel dressing.
Example 8
The acrylic acid of this comparative example was not treated with the Acer aculeatum extract, and the specific treatment was as follows:
the biological hydrogel dressing is prepared from the following raw materials in parts by weight: 1 part of hydrogel and 1.2 parts of simethicone; the hydrogel is prepared from the following raw materials in parts by weight: 30 parts of acrylic acid, 2 parts of chitosan, 1 part of a cross-linking agent, 0.5 part of a photoinitiator, 66 parts of purified water and 2 parts of a thickening agent; the preparation method of the biological hydrogel dressing comprises the following steps:
1. preparation of the biological hydrogel: a. taking 30 parts of acrylic acid, 2 parts of chitosan and 66 parts of purified water, heating and stirring to dissolve and uniformly mix, wherein the heating temperature is controlled at 60 ℃, the stirring speed is 120 r/min, and the stirring time is 20min; b. then adding 2 parts of thickener and 1 part of cross-linking agent, and continuously stirring for 20min by 0.5 part of photoinitiator; c. after the mother solution is stirred uniformly, transferring the mother solution to surface dishes, adding 12ml of the solution into each surface dish, prepolymerizing for 30min at 40 ℃, and then curing by using an ultraviolet curing box, wherein the curing parameters are as follows: the curing time is 90min at 12W and 365nm, and the improved biological hydrogel can be obtained after the curing is completed.
2. Preparation of a biological hydrogel dressing: a. shearing the cured biological hydrogel, and drying in a vacuum drying oven at 65 ℃ for 180min; b. the dried biological hydrogel fragments are put into a ball mill for grinding, and the working parameters of the mill are as follows: 30Hz,720 seconds; c. the ground gel powder passes through a 150-mesh sieve to obtain modified biological hydrogel powder; d. and uniformly mixing the ground hydrogel powder with 30 parts of simethicone to obtain the modified biological hydrogel dressing.
The cross-linking agent is: acrylic acid-N-hydroxysuccinimide ester;
the photoinitiator is as follows: alpha-ketoglutaric acid;
the thickener is as follows: gelatin
The preparation process of the biological hydrogel dressing comprises the following steps: 1. adding the hydrogel solution into a beaker, adding chitosan, and stirring the purified water for 20min;4. adding acrylic acid-N-hydroxysuccinimide ester, alpha-ketoglutaric acid and gelatin into the chamber after stirring is completed, and continuously maintaining stirring for 20min;5. uniformly stirring, transferring to a surface dish, prepolymerizing for 30min at 40 ℃, and transferring to an ultraviolet curing box for ultraviolet curing; 6. after solidification, the hydrogel is sheared, dried, ground and sieved, and is mixed with the simethicone, thus obtaining the target biological hydrogel dressing.
Test examples
The hydrogel dressings prepared in examples 1 to 8 were examined respectively for the following detection indexes: blocking strength, wherein shear stretching is measured according to YY/T0729.1-2009, T-peel stretching is measured according to YY/T0729.2-2009, and tensile strength is measured according to YY/T0729.3-2009; cytotoxicity was detected according to GB/T16886.5-2017; the bacteriostasis rate is according to WS/T650-2019; hemostatic time was measured according to YY/T1477.5-2020 standard. The results of the performance test are shown in Table 1.
Table 1 example performance test results
As can be seen from the above table, the prepared composite modified biological hydrogel dressing prepared in examples 1-5 has high antibacterial rate, short hemostatic time, high hemostatic speed, excellent adhesive strength performance such as shearing and stretching, T-stripping and stretching, tensile strength and low cytotoxicity.
In example 6, since the content of the modified acrylic acid added is low, the contact rate between the acrylic acid powders becomes low when the content of the acrylic acid powder is low due to the molecular motion principle and the time for re-gelation on the tissue surface becomes long when the powder obtained after colloid milling is coated on the tissue surface.
Whereas for example 7, since the modified acrylic acid content is too high, the probability of the crosslinking agent to attach to the polymer main chain becomes low, so that the number of NHS groups introduced thereto becomes low and the number of bonds directly affecting covalent crosslinking of the hydrogel powder with primary amine groups present on the tissue surface becomes small, resulting in a low blocking strength.
The acrylic acid added in example 8 was not treated with the Acer aculeatum extract, and the antibacterial rate was significantly reduced. According to the invention, the modified acrylic ester is prepared from the Acer aculeatum extract, so that the polyacrylic acid hydrogel dressing has better antibacterial, bacteriostatic and hemostatic capabilities, and meanwhile, the carboxyl of the modified polyacrylic acid hydrogel dressing has esterification reaction with the hydroxyl in the Acer aculeatum extract, so that the damage of the oxidization of the carboxyl to tissues and blood is greatly reduced.
In conclusion, the composite modified biological hydrogel dressing is prepared by modifying the acrylic acid. The modified hydrogel dressing of the invention not only greatly improves the adhesion strength performance of biological tissues, but also improves the biocompatibility, and has excellent application prospect when being applied to the hemostasis experiment of an in-vitro model in a simulation manner.
Claims (4)
1. The composite modified biological hydrogel dressing is characterized by comprising the following raw materials in parts by weight: 1-5 parts of modified hydrogel and 1.2-6 parts of simethicone;
the modified hydrogel is prepared from the following raw materials in parts by weight: 10-30 parts of modified acrylic acid, 1-2 parts of chitosan, 0.5-1 part of cross-linking agent, 0.25-1 part of photoinitiator, 66-89 parts of purified water and 1-2 parts of thickener;
the modified acrylic acid is prepared from the following raw materials in parts by weight: 2-5 parts of acrylic acid, 1-3 parts of a Acer aculeatum extract, 5-7 parts of a solid catalyst and 1-2 parts of a polymerization inhibitor; preparation of the modified acrylic acid: a. adding 2-5 parts of acrylic acid and 1-3 parts of Acer aculeatum extract into a container according to parts by weight, transferring into an oil bath, starting stirring under the protection of nitrogen or inert gas, controlling the rotating speed at 100-120 r/min, and uniformly stirring; b. adding 5-7 parts of solid catalyst and 1-2 parts of polymerization inhibitor; c. after being uniformly mixed, the heating temperature is started and controlled at 110-135 ℃, and the reaction time is controlled at 300-500min; c. after the reaction is completed, cooling the mixture to room temperature, and filtering insoluble substances to obtain modified acrylic acid;
The preparation of the Acer aculeatum extract comprises the following steps: a. 1-5 parts of dried and crushed Acer aculeatum branches and leaves in the shade, 4-20 parts of 94-96% v/v ethanol solution is added, soaking is carried out for 48-72 hours, the leaching solution is collected and repeated for 2-5 times, and the leaching solution is combined; b. distilling the leaching solution at 40-60deg.C under reduced pressure for 8-10 hr to obtain extract; c. vacuum drying the extract at 40-50deg.C for 48-72 hr to obtain Acer aculeatum extract;
preparation of the modified biological hydrogel: a. taking 10-30 parts of modified acrylic acid, 1-2 parts of chitosan and 66-89 parts of purified water according to parts by weight, heating and stirring to dissolve and uniformly mix, wherein the heating temperature is controlled at 40-60 ℃, the stirring speed is 120-180 r/min, and the stirring time is 10-20min; b. then adding 1-2 parts of thickener, 0.5-1 part of cross-linking agent and 0.25-1 part of photoinitiator, and continuously stirring for 10-20min; c. after the mixture is stirred uniformly, the mixture is transferred to surface dishes, 6-12ml of the solution is added into each surface dish, the mixture is prepolymerized for 30-60min at 30-40 ℃, and then the mixture is cured by an ultraviolet curing box, wherein the curing parameters are as follows: 10-15W,345-365nm, curing time of 60-120min, and obtaining the modified biological hydrogel after curing is completed;
the solid catalyst used is PW12; the polymerization inhibitor is phenothiazine; the cross-linking agent is adipic acid-N-hydroxysuccinimide; the photoinitiator is alpha-ketoglutaric acid; the thickener is gelatin.
2. The composite modified biological hydrogel dressing of claim 1, wherein the modified biological hydrogel is prepared by the following steps: a. according to the weight parts, 30 parts of modified acrylic acid, 2 parts of chitosan and 66 parts of purified water are taken, heated and stirred to be dissolved and uniformly mixed, the heating temperature is controlled at 60 ℃, the stirring speed is 120 r/min, and the stirring time is 20min; b. then adding 2 parts of thickener, 1 part of cross-linking agent and 1 part of photoinitiator, and continuously stirring for 20min; c. after it was stirred well, it was transferred to a petri dish, each petri dish was filled with 12ml of the above solution, prepolymerized at 40℃for 30min, and then cured using an ultraviolet curing oven with curing parameters: 12W,365nm, the curing time is 90min, and the modified biological hydrogel can be obtained after curing is completed.
3. The process for preparing the composite modified biological hydrogel dressing according to claim 1, comprising the following steps: a. cutting the cured modified biological hydrogel, and drying in a vacuum drying oven at 50-65deg.C for 120-180min; b. the dried biological hydrogel fragments are put into a ball mill for grinding, and the working parameters of the mill are as follows: 30-50Hz,720-1080 seconds; c. the ground gel powder is sieved by a 100-150 mesh sieve to obtain modified biological hydrogel powder; d. and uniformly mixing the ground hydrogel powder with simethicone to obtain the modified biological hydrogel dressing.
4. The process for preparing a composite modified biological hydrogel dressing as claimed in claim 3, comprising the steps of: a. cutting the cured modified biological hydrogel, and drying in a vacuum drying oven at 65 ℃ for 180min; b. the dried biological hydrogel fragments are put into a ball mill for grinding, and the working parameters of the mill are as follows: 30Hz,720 seconds; c. passing the ground gel powder through a 150-mesh sieve to obtain biological hydrogel powder; d. and uniformly mixing the ground hydrogel powder with simethicone to obtain the modified biological hydrogel dressing.
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| CN107454851A (en) * | 2015-02-16 | 2017-12-08 | 佩特洛·安德里洛维奇·曼诺瑞克 | Hemostatic composition and hemostasis device（Variant） |
| CN108159195A (en) * | 2018-01-16 | 2018-06-15 | 广西壮族自治区中国科学院广西植物研究所 | A kind of Leaf of Longestapex Beautyberry extract, preparation method and applications |
| CN110075342A (en) * | 2019-03-19 | 2019-08-02 | 邦丽达(福建)新材料股份有限公司 | A kind of high water-absorbent resin composition of antibacterial and deodouring |
| CN114767919A (en) * | 2022-04-20 | 2022-07-22 | 华中科技大学 | Hydrogel powder for rapid hemostasis and preparation method and application thereof |
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| CN107454851A (en) * | 2015-02-16 | 2017-12-08 | 佩特洛·安德里洛维奇·曼诺瑞克 | Hemostatic composition and hemostasis device（Variant） |
| CN108159195A (en) * | 2018-01-16 | 2018-06-15 | 广西壮族自治区中国科学院广西植物研究所 | A kind of Leaf of Longestapex Beautyberry extract, preparation method and applications |
| CN110075342A (en) * | 2019-03-19 | 2019-08-02 | 邦丽达(福建)新材料股份有限公司 | A kind of high water-absorbent resin composition of antibacterial and deodouring |
| CN114767919A (en) * | 2022-04-20 | 2022-07-22 | 华中科技大学 | Hydrogel powder for rapid hemostasis and preparation method and application thereof |
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